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Fumaric Acid → N-[(6R,7S)-7-(3,4-dichlorophenyl)-1,4-oxazepan-6-yl]acetamide monofumarate

HRID 1022621
ノート
印刷プレビュー

反応式

HRID 1022621 の反応式
[C:1]([NH:4][C@H:5]1[C@H:11]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=2)[O:10][CH2:9][CH2:8][N:7](C(OC(C)(C)C)=O)[CH2:6]1)(=[O:3])[CH3:2].C(OCC)(=O)C.Cl.[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]/[C:37]([OH:39])=[O:38]>C(O)C>[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]/[C:37]([OH:39])=[O:38].[Cl:19][C:14]1[CH:13]=[C:12]([C@@H:11]2[O:10][CH2:9][CH2:8][NH:7][CH2:6][C@H:5]2[NH:4][C:1](=[O:3])[CH3:2])[CH:17]=[CH:16][C:15]=1[Cl:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 444972Fumaric AcidHCID 21866389Hydrogen chloride-ethyl acetateHCID 66975754tert-butyl (6R,7S)-6-(acetylamino)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate

生成物 1

HCID 86663854N-[(6R,7S)-7-(3,4-dichlorophenyl)-1,4-oxazepan-6-yl]acetamide monofumarate収率 106.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To tert-butyl (6R,7S)-6-(acetylamino)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (200 mg) was added 4.0 M hydrogen chloride-ethyl acetate solution (4 mL), and the mixture was stirred at room temperature for 1 hr. The residue obtained by concentration under reduced pressure was desalted by a solid phase extraction resin (column: PL StrastoSphere solid phase extraction resin (PL-HCO3 MP StratoSpheres™), 500 mg, StrastoSphere, mobile phase: methanol). To a solution of the residue obtained by concentration under reduced pressure in ethanol was added a solution of fumaric acid (33.7 mg) in ethanol. The mixture was concentrated under reduced pressure to give the title compound (130 mg).

後処理

  1. customThe residue obtained by concentration under reduced pressure
  2. extractionwas desalted by a solid phase extraction resin (column
  3. extractionPL StrastoSphere solid phase extraction resin (PL-HCO3 MP StratoSpheres™), 500 mg
  4. customTo a solution of the residue obtained by concentration under reduced pressure in ethanol
  5. concentrationThe mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-8aa8d611b2354113bb13f33cf758fbdb
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722662B2

反応ノート

読み込み中…

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